CN102888750A - Method for modifying surface of carbon fiber - Google Patents
Method for modifying surface of carbon fiber Download PDFInfo
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- CN102888750A CN102888750A CN2012104207308A CN201210420730A CN102888750A CN 102888750 A CN102888750 A CN 102888750A CN 2012104207308 A CN2012104207308 A CN 2012104207308A CN 201210420730 A CN201210420730 A CN 201210420730A CN 102888750 A CN102888750 A CN 102888750A
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Abstract
The invention provides a method for modifying the surface of a carbon fiber and relates to a surface modification method. The method mainly solves the problem that the technical problem that the properties of composite material are reduced as the surface energy of the carbon fiber is improved while the body strength of the carbon fiber is lost in the existing method for modifying the surface of the carbon fiber. The method provided by the invention comprises the steps of: firstly, carrying out surface pre-treatment on the carbon fiber; secondly, immersing the carbon fiber subjected to the surface pre-treatment into a subcritical water-potassium hypermanganate system to be subjected to surface oxidation treatment; and thirdly, cleaning and drying the oxidized carbon fiber. According to the method provided by the invention, the highest oxygen content of the surface of the carbon fiber can reach up to 22.70%, and the loss of the body strength of the carbon fiber is controlled to be within 6%, so that the method provided by the invention is applicable to the fields of space flight, automobile, traffic, building, chemical industry and the like.
Description
Technical field
The present invention relates to a kind of method of surface modification.
Background technology
The supercritical fluid technique development in recent years is rapid, and relevant research work reaps rich fruits, has represented good application prospect.As a kind of reaction medium, supercritical fluid has the unrivaled character of other media: supercritical fluid has the density of approximate liquid, has stronger dissolving, penetrating power, and high polymer is had certain swelling ability; Supercritical fluid has the low viscosity of gas, easily spreads and shrinks; The solubility of supercritical fluid is closely related with density, can control it to the solvability of organic substance by the density of control fluid.These characteristics make it to become the perfect medium of a kind of material preparation and modification, show huge using value at aspects such as the manufacturing of fiber and modifications.
Carbon fiber is a kind of existing structure load-bearing effect, has again functional material.Be widely used in fields such as space flight, automobile, traffic, building, chemical industry in recent years.Undressed carbon fiber surface activity group is few, and surface inertness is large, and is poor with matrix compound tense Interface adhesive strength, has more boundary defect.These problems have all limited the advantage performances such as the high strength, high ratio modulus of carbon fiber greatly.Therefore carbon fiber surface being processed, is to promote carbon fiber to use the key of development.At present, the research of carbon fiber processing method has a lot, mainly concentrates on carbon fiber surface is processed, and make its surface have active group or improve its surface roughness, and then the adhesive strength of raising and matrix.Surface treatment method mainly is divided into oxidizing process and non-oxide method two large classes.Method relatively more commonly used has electrochemical deposition method, liquid phase oxidation, vapour phase oxidation process, plasma method and radiation graft process etc. now.These methods have also been lost carbon fiber in the surface property that improves carbon fiber body intensity, and oxidation is uneven, and oxidation effectiveness is bad, causes its final composite property to reduce.
Summary of the invention
The present invention will solve the body intensity of also having lost carbon fiber when improving carbon fibre surface energy that the method for existing carbon fiber surface modification exists, cause the technical problem of its final composite property reduction, thereby a kind of method of carbon fiber surface modification is provided.
A kind of method of carbon fiber surface modification is to carry out according to the following steps:
One, carbon fiber bundle is carried out surface preparation: carbon fiber bundle is put into extraction device, in acetone behind 75～85 ℃ of extracting 4～6h, carbon fiber bundle is put into overcritical device, in overcritical acetone-water system, soak 20～30min in 360～370 ℃, carbon fiber bundle is carried out further surface clean, the carbon fiber bundle that to process is again put into extraction device again, in acetone in 75～85 ℃ of extracting 2～4h.
Two, will the carbon fiber bundle after the surface preparation immerse and carry out surface oxidation treatment in subcritical water-potassium permanganate system: in 30～40ml molar concentration is the sulfuric acid of 1～1.5mol/L, add 0.2～0.5g potassium permanganate preparation oxidation solution, to put into test tube through the carbon fiber bundle after the step 1 surface preparation, make oxidation solution submergence carbon fiber bundle, again test tube is put into reactor, reactor is put into overcritical device, after reacting 20～30min under 320～330 ℃ of conditions, take out reactor, make it to naturally cool to room temperature.
Three, carbon fiber bundle after the oxidation is carried out cleaning-drying: open reactor, take out the carbon fiber bundle in the test tube, use distilled water flushing, after the flushing, carbon fiber bundle is put into extraction device, in acetone in 75～85 ℃ of extracting 2～4h, it is that 36%～38% concentrated hydrochloric acid adds hot reflux 2～4h under 80～90 ℃ of conditions that carbon fiber bundle is put into mass concentration, making potassium permanganate on the carbon fiber bundle and mass concentration is that 36%～38% concentrated hydrochloric acid reaction generates chlorine, remove potassium permanganate residual on the fiber, then take out carbon fiber bundle, with the distilled water flushing carbon fiber bundle until after liquid is neutrality after the flushing, carbon fiber bundle is put into 70～90 ℃ of baking oven 18～24h.
The present invention includes following effect:
The present invention is by the preliminary treatment of carbon fiber surface, subcritical water-potassium permanganate system is carried out oxidation to carbon fiber, the steps such as cleaning to carbon fiber after the oxidation have been carried out modification to carbon fiber surface, make the oxygen content of carbon fiber surface 15.98%～22.70%, and can keep the damage control to carbon fiber body intensity in 6%, solved the body intensity of in the surface property that improves carbon fiber, also having lost carbon fiber that exists in the existing carbon fiber surface modification method, the problem that causes its final composite property to reduce, simultaneously, also make the fiber surface oxidation even, effect is better than the nitration mixture oxidation.
Description of drawings
Fig. 1 is the full spectrogram of the XPS of precursor;
Fig. 2 is the full spectrogram of XPS of carbon fiber after the 0.2g potassium permanganate oxidation liquid oxidation oxidation in the test one;
Fig. 3 is the full spectrogram of XPS of carbon fiber after the 0.3g potassium permanganate oxidation liquid oxidation oxidation in the test two;
Fig. 4 is the full spectrogram of XPS of carbon fiber after the 0.35g potassium permanganate oxidation liquid oxidation oxidation in the test three;
Fig. 5 is the full spectrogram of XPS of carbon fiber after the potassium permanganate oxidation liquid oxidation oxidation among the 0.4g in the test four;
Fig. 6 is the full spectrogram of XPS of carbon fiber after the 0.5g potassium permanganate oxidation liquid oxidation oxidation in the test five;
Fig. 7 is the SEM picture of precursor;
Fig. 8 is the SEM picture that test one contains carbon fiber after the liquid oxidation of 0.2g potassium permanganate oxidation;
Fig. 9 is the SEM picture that test two contains carbon fiber after the liquid oxidation of 0.3g potassium permanganate oxidation;
Figure 10 is the SEM picture that test three contains carbon fiber after the liquid oxidation of 0.35g potassium permanganate oxidation;
Figure 11 is the SEM picture that test four contains carbon fiber after the liquid oxidation of 0.4g potassium permanganate oxidation;
Figure 12 is the SEM picture that test five contains carbon fiber after the liquid oxidation of 0.5g potassium permanganate oxidation;
Figure 13 is the C1 s of carbon fiber spectrum swarming after the liquid oxidation of 0.5g potassium permanganate oxidation in the test five.
The specific embodiment
The specific embodiment one: a kind of method of carbon fiber surface modification is carried out according to the following steps in the present embodiment:
One, carbon fiber bundle is carried out surface preparation: carbon fiber bundle is put into extraction device, in acetone behind 75～85 ℃ of extracting 4～6h, carbon fiber bundle is put into overcritical device, in overcritical acetone-water system, soak 20～30min in 360～370 ℃, carbon fiber bundle is carried out further surface clean, the carbon fiber bundle that to process is again put into extraction device again, in acetone in 75～85 ℃ of extracting 2～4h.
Two, will the carbon fiber bundle after the surface preparation immerse and carry out surface oxidation treatment in subcritical water-potassium permanganate system: in 30～40ml molar concentration is the sulfuric acid of 1～1.5mol/L, add 0.2～0.5g potassium permanganate preparation oxidation solution, to put into test tube through the carbon fiber bundle after the step 1 surface preparation, make oxidation solution submergence carbon fiber bundle, again test tube is put into reactor, reactor is put into overcritical device, after reacting 20～30min under 320～330 ℃ of conditions, take out reactor, make it to naturally cool to room temperature.
Three, carbon fiber bundle after the oxidation is carried out cleaning-drying: open reactor, take out the carbon fiber bundle in the test tube, use distilled water flushing, after the flushing, carbon fiber bundle is put into extraction device, in acetone in 75～85 ℃ of extracting 2～4h, it is that 36%～38% concentrated hydrochloric acid adds hot reflux 2～4h under 80～90 ℃ of conditions that carbon fiber bundle is put into mass concentration, making potassium permanganate on the carbon fiber bundle and mass concentration is that 36%～38% concentrated hydrochloric acid reaction generates chlorine, remove potassium permanganate residual on the fiber, then take out carbon fiber bundle, with the distilled water flushing carbon fiber bundle until after liquid is neutrality after the flushing, carbon fiber bundle is put into 70～90 ℃ of baking oven 18～24h.
Present embodiment comprises following effect:
Present embodiment is by the preliminary treatment of carbon fiber surface, subcritical water-potassium permanganate system is carried out oxidation to carbon fiber, the steps such as cleaning to carbon fiber after the oxidation have been carried out modification to carbon fiber surface, make the oxygen content of carbon fiber surface reach as high as 22.70%, and can keep the damage control to carbon fiber body intensity in 6%, solved the body intensity of in the surface property that improves carbon fiber, also having lost carbon fiber that exists in the existing carbon fiber surface modification method, the problem that causes its final composite property to reduce, simultaneously, also make the fiber surface oxidation even, effect is better than the nitration mixture oxidation.
The specific embodiment two: what present embodiment and the specific embodiment one were different is: soak 20min in 360 ℃ in the step 1 in overcritical acetone-water system.Other is identical with the specific embodiment one.
The specific embodiment three: what present embodiment was different from the specific embodiment one or two is: react 20min in the step 2 under 320 ℃ of conditions.Other is identical with the specific embodiment one or two.
The specific embodiment four: what present embodiment was different from one of specific embodiment one to three is: in the step 3 carbon fiber bundle is put into extraction device, in acetone in 80 ℃ of extracting 2h.Other is identical with one of specific embodiment one to three.
The specific embodiment five: what present embodiment was different from one of specific embodiment one to four is: in the step 3 carbon fiber bundle put into mass concentration and be 36%～38% concentrated hydrochloric acid and add hot reflux 2h under 80 ℃ of conditions.Other is identical with one of specific embodiment one to four.
The specific embodiment six: what present embodiment was different from one of specific embodiment one to five is: in the step 3 fibre bundle is put into 80 ℃ of baking ovens and dry 24h.Other is identical with one of specific embodiment one to five.
By following verification experimental verification beneficial effect of the present invention:
Test one: the method for a kind of carbon fiber surface modification of this test is to realize by the following method:
One, carbon fiber bundle is carried out surface preparation: carbon fiber bundle is put into extraction device, in acetone behind 80 ℃ of extracting 4h, carbon fiber bundle is put into overcritical device, in overcritical acetone-water system, soak 20min in 360 ℃, carbon fiber bundle is carried out further surface clean, the carbon fiber bundle that to process is again put into extraction device again, in acetone in 80 ℃ of extracting 2h.
Two, will the carbon fiber bundle after the surface preparation immerse and carry out surface oxidation treatment in subcritical water-potassium permanganate system: in the 35ml molar concentration is the sulfuric acid of 1mol/L, add 0.2g potassium permanganate preparation oxidation solution, to put into test tube through the carbon fiber bundle after the step 1 surface preparation, make oxidation solution submergence carbon fiber bundle, again test tube is put into reactor, reactor is put into overcritical device, behind reaction 20min under 320 ℃ of conditions, take out reactor, make it to naturally cool to room temperature.
Three, carbon fiber bundle after the oxidation is carried out cleaning-drying: open reactor, take out the carbon fiber bundle in the test tube, use distilled water flushing, after the flushing, carbon fiber bundle is put into extraction device, in acetone in 80 ℃ of extracting 2h, it is that 36.5% concentrated hydrochloric acid adds hot reflux 2h under 80 ℃ of conditions that carbon fiber bundle is put into mass concentration, making potassium permanganate on the carbon fiber bundle and mass concentration is that 36.5% concentrated hydrochloric acid reaction generates chlorine, remove potassium permanganate residual on the fiber, then take out carbon fiber bundle, with the distilled water flushing carbon fiber bundle until after liquid is neutrality after the flushing, carbon fiber bundle is put into 80 ℃ of baking oven 24h.
In this test one after the 0.2g potassium permanganate oxidation liquid oxidation oxidation the full spectrogram of XPS of carbon fiber the O1s peak is arranged in conjunction with being positioned at about 533eV as can be seen from Figure 2, and the O1s peak is than the O1s peak height of the full spectrogram of XPS of Fig. 1 precursor as shown in Figure 2;
The SEM picture that this test one contains carbon fiber after the liquid oxidation of 0.2g potassium permanganate oxidation as shown in Figure 8, oxidation has played certain corrasion to carbon fiber surface as can be seen from Figure 8, the groove of carbon fiber surface is deepened, and groove is deeper than the groove of the SEM picture of Fig. 7 precursor.
Test two: the method for a kind of carbon fiber surface modification of this test is to realize by the following method: this test and test one are different to be: adding 0.3g potassium permanganate is prepared oxidation solution among a of step 2, and other processes and parameter are identical with test one.
In this test two after the 0.3g potassium permanganate oxidation liquid oxidation oxidation the full spectrogram of XPS of carbon fiber as shown in Figure 3, as can be seen from Figure 3 in conjunction with being positioned at O1s peak about 533eV than the O1s peak height of Fig. 2;
The SEM picture that this test two contains carbon fiber after the liquid oxidation of 0.3g potassium permanganate oxidation as shown in Figure 9, oxidation has played certain corrasion to carbon fiber surface as can be seen from Figure 9, the groove of carbon fiber surface is deepened, and groove is darker than Fig. 8.
Test three: the method for a kind of carbon fiber surface modification of this test is to realize by the following method: this test and test one are different to be: adding 0.35g potassium permanganate is prepared oxidation solution among a of step 2, and other processes and parameter are identical with test one.
In this test three after the 0.35g potassium permanganate oxidation liquid oxidation oxidation the full spectrogram of XPS of carbon fiber as shown in Figure 4, as can be seen from Figure 4 in conjunction with being positioned at O1s peak about 533eV than the O1s peak height of Fig. 3;
The SEM picture that this test three contains carbon fiber after the liquid oxidation of 0.35g potassium permanganate oxidation as shown in figure 10, oxidation has played certain corrasion to carbon fiber surface as can be seen from Figure 10, the groove of carbon fiber surface is deepened, and groove is darker than Fig. 9.
Test four: the method for a kind of carbon fiber surface modification of this test is to realize by the following method: this test and test one are different to be: adding 0.4g potassium permanganate is prepared oxidation solution among a of step 2, and other processes and parameter are identical with test one.
In this test four after the 0.4g potassium permanganate oxidation liquid oxidation oxidation the full spectrogram of XPS of carbon fiber as shown in Figure 5, as can be seen from Figure 5 in conjunction with being positioned at O1s peak about 533eV than the O1s peak height of Fig. 4;
The SEM picture that this test four contains carbon fiber after the liquid oxidation of 0.4g potassium permanganate oxidation as shown in figure 11, oxidation has played certain corrasion to carbon fiber surface as can be seen from Figure 11, the groove of carbon fiber surface is deepened, and groove is darker than Figure 10.
Test five: the method for a kind of carbon fiber surface modification of this test is to realize by the following method: this test and test one are different to be: adding 0.5g potassium permanganate is prepared oxidation solution among a of step 2, and other processes and parameter are identical with test one.
In this test five after the 0.5g potassium permanganate oxidation liquid oxidation oxidation the full spectrogram of XPS of carbon fiber as shown in Figure 6, as can be seen from Figure 6 in conjunction with being positioned at O1s peak about 533eV than the O1s peak height of Fig. 5;
The SEM picture that this test five contains carbon fiber after the liquid oxidation of 0.5g potassium permanganate oxidation as shown in figure 12, oxidation has played certain corrasion to carbon fiber surface as can be seen from Figure 12, the groove of carbon fiber surface is deepened, and groove is darker than Figure 11;
The C1s of carbon fiber spectrum swarming is as shown in figure 13 after the liquid oxidation of 0.5g potassium permanganate oxidation in this test five, be positioned at as can be seen from Figure 13 near the 288.4eV-the COOH overshooting goes out obviously, also occurred-the COH peak near being positioned at 286.0eV, illustrate after the oxidation fiber surface produced a large amount of-COOH and-COH,-COOH and-generation of COH, can significantly improve the surface energy of carbon fiber, strengthen resin to the wettability of carbon fiber, improve the interface bond strength of carbon fiber and epoxy resin.
By above-mentioned test as can be known:
1, along with the rising of potassium permanganate content in the oxidation solution, uprise gradually in conjunction with the O1s peak that can be positioned at about 533eV, namely the oxygen content of oxidized fibre raises gradually along with the rising of potassium permanganate content in the oxidation solution;
2, oxidation has played certain corrasion to carbon fiber surface, the groove of carbon fiber surface is deepened, and along with the increasing of potassium permanganate content, this corrasion is more and more obvious, " rivet " effect that this can strengthen carbon fiber and epoxy resin compound tense improves the interface combination.
The surface-element content distribution table of precursor and carbon oxide fiber is as shown in table 1, data show in the table 1: along with the raising of potassium permanganate content, the oxygen content of carbon fiber surface improves gradually, elevated oxygen level can reach 22.7%, show that namely adding potassium permanganate in subcritical water carries out the oxygen content that energy of oxidation significantly improves carbon fiber surface to carbon fiber, obviously improves its surperficial oxy radical number.
Table 1
The monofilament tensile strength of carbon fiber is as shown in table 2 after precursor and the oxidation, table 2 data show: the loss of the filament strength of fiber remains in 6% after the oxidation, illustrate that oxidizing process does not cause large destruction to fiber bodies, the body intensity of carbon fiber is substantially constant.
Table 2
The surface energy of carbon fiber is as shown in table 3 after precursor and the oxidation, and table 3 data show: along with the raising of potassium permanganate content in the system, the surface energy of carbon fiber improves gradually after the oxidation.The raising of carbon fibre surface energy can significantly improve the impregnation process of itself and epoxy resin, makes infiltration more evenly fully.
Table 3
Claims (6)
1. the method for a carbon fiber surface modification is characterized in that the method for carbon fiber surface modification is carried out according to the following steps:
One, carbon fiber bundle is carried out surface preparation: carbon fiber bundle is put into extraction device, in acetone behind 75～85 ℃ of extracting 4～6h, carbon fiber bundle is put into overcritical device, in overcritical acetone-water system, soak 20～30min in 360～370 ℃, carbon fiber bundle is carried out further surface clean, the carbon fiber bundle that to process is again put into extraction device again, in acetone in 75～85 ℃ of extracting 2～4h.
Two, will the carbon fiber bundle after the surface preparation immerse and carry out surface oxidation treatment in subcritical water-potassium permanganate system: in 30～40ml molar concentration is the sulfuric acid of 1～1.5mol/L, add 0.2～0.5g potassium permanganate preparation oxidation solution, to put into test tube through the carbon fiber bundle after the step 1 surface preparation, make oxidation solution submergence carbon fiber bundle, again test tube is put into reactor, reactor is put into overcritical device, after reacting 20～30min under 320～330 ℃ of conditions, take out reactor, make it to naturally cool to room temperature.
Three, carbon fiber bundle after the oxidation is carried out cleaning-drying: open reactor, take out the carbon fiber bundle in the test tube, use distilled water flushing, after the flushing, carbon fiber bundle is put into extraction device, in acetone in 75～85 ℃ of extracting 2～4h, it is that 36%～38% concentrated hydrochloric acid adds hot reflux 2～4h under 80～90 ℃ of conditions that carbon fiber bundle is put into mass concentration, making potassium permanganate on the carbon fiber bundle and mass concentration is that 36%～38% concentrated hydrochloric acid reaction generates chlorine, remove potassium permanganate residual on the fiber, then take out carbon fiber bundle, with the distilled water flushing carbon fiber bundle until after liquid is neutrality after the flushing, carbon fiber bundle is put into 70～90 ℃ of baking oven 18～24h.
2. the method for a kind of carbon fiber surface modification according to claim 1 is characterized in that soaking 20min in 360 ℃ in the step 1 in overcritical acetone-water system.
3. the method for a kind of carbon fiber surface modification according to claim 1 is characterized in that reacting 20min in the step 2 under 320 ℃ of conditions.
4. the method for a kind of carbon fiber surface modification according to claim 1 is characterized in that in the step 3 carbon fiber bundle being put into extraction device, in acetone in 80 ℃ of extracting 2h.
5. the method for a kind of carbon fiber surface modification according to claim 1 is characterized in that in the step 3 carbon fiber bundle put into mass concentration and is 36%～38% concentrated hydrochloric acid and add hot reflux 2h under 80 ℃ of conditions.
6. the method for a kind of carbon fiber surface modification according to claim 1 is characterized in that in the step 3 fibre bundle being put into 80 ℃ of baking ovens dries 24h.
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| CN103469534A (en) * | 2013-09-30 | 2013-12-25 | 哈尔滨工业大学 | Method for chemical grafting modification for surfaces of carbon fibers |
| CN103469534B (en) * | 2013-09-30 | 2015-05-13 | 哈尔滨工业大学 | Method for chemical grafting modification for surfaces of carbon fibers |
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| CN107034662A (en) * | 2017-04-10 | 2017-08-11 | 中国铝业股份有限公司 | A kind of method of carbon fiber surface modification |
| CN110423367A (en) * | 2019-08-14 | 2019-11-08 | 哈尔滨工业大学 | A kind of preparation method of fibre reinforced thermoplastic composite |
| CN110423367B (en) * | 2019-08-14 | 2022-04-08 | 哈尔滨工业大学 | Preparation method of carbon fiber reinforced thermoplastic composite material |
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